Effect of different lipid extraction methods on δ13C of lipid and lipid-free fractions of fish and different fish feeds

For many ecological applications of stable carbon isotope techniques, it is necessary to separate the lipid and lipid-free fractions. The effect of different lipid extraction methods on the isotope signature of the remaining lipid-free matter as well as the lipid fraction was tested. A hot extraction form of the Soxhlet method using petrol-ether was compared with two liquid-liquid extraction methods for lipid determination described by Bligh and Dyer and Smedes. Solid samples of fish and different natural food items were subjected to extraction and the carbon isotope ratios in lipid and lipid-free matter determined by IRMS. All methods were suitable for lipid extraction from all samples analysed here and did not cause biologically relevant differences (>1) in carbon isotopic ratios, except the Bligh and Dyer extraction method using chloroform which caused systematic errors for δ ¹³C when applied to diatoms.     

Effect of different lipid extraction methods on delta13C of lipid and lipid-free fractions of fish and different fish feeds

For many ecological applications of stable carbon isotope techniques, it is necessary to separate the lipid and lipid-free fractions. The effect of different lipid extraction methods on the isotope signature of the remaining lipid-free matter as well as the lipid fraction was tested. A hot extraction form of the Soxhlet method using petrol-ether was compared with two liquid-liquid extraction methods for lipid determination described by Bligh and Dyer and Smedes. Solid samples of fish and different natural food items were subjected to extraction and the carbon isotope ratios in lipid and lipid-free matter determined by IRMS. All methods were suitable for lipid extraction from all samples analysed here and did not cause biologically relevant differences (> 1%) in carbon isotopic ratios, except the Bligh and Dyer extraction method using chloroform which caused systematic errors for delta13C when applied to diatoms.     

Effect of drying technique on the physicochemical properties of sodium silicate-based mesoporous precipitated silica

The conventional drying (oven drying) method used for the preparation of precipitated mesoporous silica with low surface area (>300 m²/g) and small pore volume is often associated with a high production cost and a time consuming process. Therefore, the main goal of this study was to develop a cost-effective and fast drying process for the production of precipitated mesoporous silica using inexpensive industrial grade sodium silicate and spray drying of the precipitated wet-gel silica slurry. The precipitated wet-gel silica slurry was prepared from an aqueous sodium silicate solution through the drop-wise addition of sulfuric acid. Mesoporous precipitated silica powder was prepared by drying the wet-gel slurry with different drying techniques. The effects of the oven drying (OD), microwave drying (MD), and spray drying (SD) techniques on the physical (oil, water absorption, and tapping density), and textural properties (specific BET surface area, pore volume, pore size, and % porosity) of the precipitated mesoporous silica powder were studied. The dried precipitated mesoporous silica powders were characterized with field-emission scanning electron microscopy; Brunauer, Emmett and Teller and BJH nitrogen gas adsorption/desorption methods; Fourier-transform infrared spectroscopy; thermogravimetric and differential analysis; N₂ physisorption isotherm; pore size distribution and particle size analysis. There was a significant effect of drying technique on the textural properties, such as specific surface area, pore size distribution and cumulative pore volume of the mesoporous silica powder. Additionally, the effect of the microwave-drying period on the physicochemical properties of the precipitated mesoporous silica powder was investigated and discussed.     

Optimization of ultrasonic-assisted extraction of pomegranate (Punica granatum L.) seed oil

The effectiveness of ultrasonic-assisted extraction (UAE) of pomegranate seed oil (PSO) was evaluated using a variety of solvents. Petroleum ether was the most effective for oil extraction, followed by n-hexane, ethyl acetate, diethyl ether, acetone, and isopropanol. Several variables, such as ultrasonic power, extraction temperature, extraction time, and the ratio of solvent volume and seed weight (S/S ratio) were studied for optimization using response surface methodology (RSM). The highest oil yield, 25.11% (w/w), was obtained using petroleum ether under optimal conditions for ultrasonic power, extraction temperature, extraction time, and S/S ratio at 140 W, 40 °C, 36 min, and 10 ml/g, respectively. The PSO yield extracted by UAE was significantly higher than by using Soxhlet extraction (SE; 20.50%) and supercritical fluid extraction (SFE; 15.72%). The fatty acid compositions were significantly different among the PSO extracted by Soxhlet extraction, SFE, and UAE, with punicic acid (>65%) being the most dominant using UAE.     

Ultrasonic pre-irradiation effect upon aqueous enzymatic oil extraction from almond and apricot seeds

The present work evaluates the benefit of using ultrasonic pre-irradiation before extracting oil from almond and apricot seeds by aqueous enzymatic oil extraction (AEOE) process. The use of a commercial preparation which is a mixture of three proteases in AEOE gave 75% w/w oil yield from almonds at pH 4.0 in 18 h at 40 °C. The ultrasonic pre-irradiation at 70 W for 2 min increased the yield to 95%, w/w and reduced the extraction time to 6 h. The effect of ultrasonic pre-irradiation on meal morphology could be visually seen by scanning electron micrographs. It indicates development of of microfractures and disruption of cell walls in almond powder. With apricot, also, ultrasonic pre-irradiation also marginally increased the oil yield obtained by AEOE to 77% w/w and reduced the extraction time to 6 h. Thus, ultrasonic pre-irradiation step may reduce time required to extract oil from edible oils from plant sources and hence can improve through put in commercial oil production process.     

Ultrasound extraction optimization for bioactive molecules from Eucalyptus globulus leaves through antioxidant activity

Antioxidant products present a very high added value and are demanded in the market. The optimization of their extraction is a high-stakes matter for both economic and environmental points of view. Ultrasound extraction has been considered one of the most promising methods, so the relative importance of key parameters may have decisive economic significance. For this reason, different parameters that have influence on the extraction capacity such as ultrasound power, time, temperature, pH and % ethanol in water have been studied to know the relationships between the independent parameters and their influence on the extraction from Eucalyptus globulus leaves. An experimental Box-Behnken factorial design and subsequent analysis by neural networks have been used. The relative influence of each parameter varies according to the nature of the extracted compound. In this regard, the higher capacity of extraction of the selected antioxidant compounds by means of the variation of the operation conditions can be facilitated. For all the studied compounds, temperature has been the most important parameter for their extraction. The relative content (%) of bioactive compounds (terpenes) in the optimized Eucalyptus globulus extract has been performed by GC–MS analysis.     

Ultrasound-assisted production of biodiesel using engineered methanol tolerant Proteus vulgaris lipase immobilized on functionalized polysulfone beads

In the present study, Proteus vulgaris lipase (PVL) was engineered using directed evolution to increase methanol tolerance so that it would be more tolerant and efficient for harsh conditions employed in biodiesel synthesis, which is limiting their industrial use. The influence of ultrasound under different experimental conditions on the biodiesel conversion yield using methanolysis of non-edible neem oil was also emphasized. A special attention was also paid to the immobilization of lipase on Polysulfone (PS) beads and comparative studies with industrially used Burkholderia cepacia lipase. The Engineered Proteus vulgaris lipase showed >80% activity after 3 h when incubated in 50% methanol with simultaneous sonication. The lipase retained improved longevity (~70% residual activity) over wild-type PVL over repeated use.     

An ammonium sulfate/ethanol aqueous two-phase system combined with ultrasonication for the separation and purification of lithospermic acid B from Salvia miltiorrhiza Bunge

We studied the effect of ultrasonication extraction technology combined with ammonium sulfate/ethanol aqueous two-phase system (ATPS) for the separation of lithospermic acid B (LAB) from Salvia miltiorrhiza Bunge. According to the literature and preliminary studies, ammonium sulfate concentration, ethanol concentration, pH, ultrasonication power, ultrasonication time and the ratio of solvent-to-solid were investigated using a single factor design to identify the factors affecting separation. Taking into consideration a simultaneous increase in LAB recovery (R (%)) and partition coefficient (K), the best performance of the ATPS was obtained at 25 °C and pH 2 using ammonium sulfate 22% (w/w) and ethanol 30% (w/w). To keep the solvent-to-solid ratio at 10, response surface methodology was used to find the optimal ultrasonication power and ultrasonication time. Quadratic models were predicted for LAB yield in the upper phase. Optimal conditions of 572.1 W ultrasonication power and 42.2 min produced a maximum yield of LAB of 42.16 mg g⁻¹ sample. There was no obvious degradation of LAB with ultrasound under the applied conditions, and the experimental yield of LAB was 42.49 mg g⁻¹ sample and the purity was 55.28% (w/w), which was much higher than that obtained using conventional extraction. The present study demonstrated that ultrasound coupled with aqueous two-phase systems is very efficient tool for the extraction and purification of LAB from Salvia miltiorrhiza Bunge.     

Effect of the ultrasound-assisted preliminary maceration on the efficiency of the essential oil distillation from selected herbal raw materials

The objective of the study was the estimation of the ultrasound-assisted preliminary maceration effect on the efficiency of essential oil distillation and on its qualitative and quantitative composition. The experiment included analyses on three herbal materials, i.e. peppermint leaves (Mentha piperita L.), marjoram herb (Origanum majorana L.), and chamomile flowers (Chamomilla recutita (L.) Rauschert). The study showed that the application of preliminary water maceration of raw material, augmented with ultrasounds, had a statistically significant increasing effect on the amount of oil distilled, in the case of mint leaf from 1.32% to 1.46% v/w, and in the case of marjoram herb from 1.13% to 1.27% v/w. In the case of chamomile flowers no significant effect of ultrasound on the amount of oil obtained was observed. Generally, comparing the composition of essential oils obtained in the experiments with the requirements of the relevant standards no unfavourable effect of the distillation augmenting techniques applied was noted. Therefore, it should be expected that the studied distillates of volatile fractions will have the desired biological activity.     

Synthesis, structural and optical characterization of nanocrystalline ZnS:Cu embedded in silica matrix

The synthesis of Cu doped ZnS nanoparticles inside the pore of an inorganic silica gel matrix is presented. The synthesized nanoparticles were characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive X-ray (EDX). X-ray diffraction pattern reveals the crystalline wurtzite phase of ZnS. The existence of silica gel in modeling morphologies of the nanoparticles was characterized using Fourier transform infrared (FTIR) spectrometer. Thickness of the silica shell was also calculated. UV- absorption spectrum shows the appearance of an absorption peak at 273 nm which confirms the blue shift as compared to that of bulk ZnS. The photoluminescence (PL) emission spectrum of the sample showed a broad band in the range 465-510 nm due to the transition from the conduction band edge of ZnS nanocrystals to the acceptor like t₂ state of Cu.     

Nanocomposites with fumed silica/poly(vinyl pyrrolidone) prepared at a low content of solvents

Highly disperse nanocomposites with fumed silica/poly(vinyl pyrrolidone) (PVP) prepared using different methods were studied by infrared spectroscopy, adsorption, and quantum chemistry methods. Low amounts of water or ethanol (30 wt.% with respect to the silica content) promote appropriate distribution of PVP on silica particles. The use of ethanol leads to a smaller loss of the specific surface area (S_BET) than in the case of water used as a solvent. On PVP distribution on a silica surface, treatment of the system in a pseudo-liquid state reactor (PLSR) provides slightly better results (a lower loss in S_BET) in comparison with mechanochemical activation (MCA) in a ball mill at the PVP monolayer coverage. An increase in the activation time to 6-9 h leads to an increase in the |ΔS_BET/S_BET| value to 0.29-0.35 for both treatment methods.     

Solvothermal removal of the organic template from L 3 (“sponge”) templated silica monoliths

We compare the methods of continuous solvent (Soxhlet) and supercritical solvent extractions for the removal of the organic template from nanostructured silica monoliths. Our monoliths are formed by templating the L ₃ liquid crystal phase of cetylpyridinium chloride in aqueous solutions with tetramethoxy silane. The monoliths that result from both Soxhlet and supercritical extraction methods are mechanically robust, optically clear, and free of cracks. The Soxhlet method compares favorably with supercritical solvent extraction in that equivalent L ₃-templated silica can be synthesized without the use of specialized reactor hardware or higher temperatures and high pressures, while avoiding noxious byproducts. The comparative effectiveness of various solvents in the Soxhlet process is related to the Hildebrand solubility parameter, determined by the effective surface area of the extracted silica.     

Aqueous two-phase system coupled with ultrasound for the extraction of lignans from seeds of Schisandra chinensis (turcz.) Baill

In this study the potential use of an aqueous two phase system (ATPS) coupled with ultrasound for the extraction of lignans from Schisandra chinensis seeds was evaluated and optimized using response surface methodology (RSM). The main bioactive components, schizandrin (SA), schisantherin A (SAA) and deoxyschizandrin (DSA) were selected as markers. The partitioning behavior of lignans in different salt-types of ATPS was compared. The optimization ATPS of 25% (w/w) (NH₄)₂SO₄ and 19% (w/w) ethanol were selected based on their higher upper phase partitioning coefficient (>74) and the recovery (>93%) for three markers. Using the optimized ATPS solvent, the RMS results showed 20:1 of solvent:solid, 800 W and 61.1 min were the optimal ultrasound assisted extraction conditions, under which 13.10 mg/g SA, 1.87 mg/g SAA and 1.84 mg/g DSA were recovered in the upper phase, whereas the wasted stigmas accumulated in the lower phase. Compared with 80% ethanol (v/v) ultrasonic extraction, similar yields were obtained, but the present method exhibited higher extraction purity for the selective extraction of lignans from S. chinensis seeds.     

Intensified recovery of lipids,proteins, and carbohydrates from wastewater-grown microalgae Desmodesmus sp. by using ultrasound or ozone

This study evaluates the effect of ultrasound and ozone pretreatments for the subsequent recovery of Desmodesmus sp. biocomponents—lipids, proteins, and carbohydrates—using a response surface methodology. Both pretreatments impact on the recovered lipids quality, solvent waste production and extraction time is analysed for process intensification purposes. For ultrasound pretreatment, independent parameters were energy applied (50–200 kWh/kg dry biomass), biomass concentration (25–75 g/L), and ultrasonic intensity (0.32 and 0.53 W/mL). While for ozone pretreatment, independent parameters were ozone concentration (3–9 mg O₃/L), biomass concentration (25–75 g/L), and contact time (5–15 min). In the case of ultrasound pretreatment, recovery yield reached 97 ± 0.4%, 89 ± 3%, and 73 ± 0.6% for proteins, carbohydrates and lipids respectively. Given process required: energy applied of 50 kWh/kg dry biomass, 75 g/L of biomass concentration, 0.32 W/mL of ultrasonic intensity, and 56 min of time process. Ultrasound caused high cell disruption releasing all proteins, thereby obviating downstream processing for its recovery. Ozone pretreatment recovery yield was 85 ± 2%, 48 ± 1.4%, and 25 ± 1.3%, for carbohydrates, lipids and proteins respectively, under the following conditions: 9 mg O₃/L of ozone concentration, 25 g/L of biomass concentration, and 5 min of contact time that depicts an energy consumption of 30.64 kWh/kg dry biomass. It was found that ultrasound and ozone pretreatments intensified the lysis and biocomponents recovery process by reducing solvent consumption by at least 92% and extraction time between 80% and 90% compared with extraction of untreated biomass biocomponents. Both pretreatments improve the composition of the recovered lipids. It was noted that the yield of neutral lipids increased from 28% to 67% for ultrasound pretreatment while for ozone pretreatment from 49% to 63%. The method used for lipid extraction may also have an effect but here it was kept constant.     

Sequential extraction and enrichment of flavonoids from Euonymus alatus by ultrasonic-assisted polyethylene glycol-based extraction coupled to temperature-induced cloud point extraction

A green method for simultaneous extraction and enrichment of flavonoids from Euonymus alatus was developed by ultrasonic-assisted extraction (UAE) and temperature-induced cloud point extraction (TICPE) using PEG-base aqueous solution as the extractant. Based on screening different molecular weights of PEGs, PEG-400/water was used as the extractant, and the effects of key factors on extraction yields of flavonoids were investigated by single-factor experiments and response surface methodology (RSM). The optimum conditions of UAE were as follows: PEG-400 concentration of 16% (w/w), particle size of 80 mesh, solvent-to-material ratio of 60:1, extraction temperature of 90 °C and extraction time of 15 min. The results obtained by validation experiments were consistent with the values predicted by RSM. Temperature-induced formation of the aqueous two-phase system (ATPS) and TICPE process were further investigated by controlling temperature and adding (NH₄)₂SO₄. In the presence of (NH₄)₂SO₄, the ATPS formed at 75 ℃ and pH 3.5 could effectively improve separation and recovery of flavonoids with enrichment factor of above five times. Gallic acid, catechin, dihydromyricetin and ellagic acid in the extract were identified and confirmed by UPLC-Q-TOF-MS and the corresponding standards. The UAE-TICPE coupled to HPLC was successfully applied for extraction and determination of flavonoids in two batches of Euonymus alatus. The extraction yields of catechin, dihydromyricetin and total flavonoids were 0.377–0.684 mg/g, 1.091–1.353 mg/g and 2.612–3.146 mg/g, respectively. Compared to conventional extraction methods, PEG-based UAE integrated with TICPE in one-step procedure exhibited higher extraction efficiency and better extraction selectivity.     

Optimization and kinetic modeling of ultrasonic-assisted extraction of fucoxanthin from edible brown algae Sargassum fusiforme using green solvents

The development of green and sustainable extraction technologies for various naturally active biomaterials is gaining increasing attention due to their environmentally friendly advantages. In this work, the ultrasonic-assisted extraction of fucoxanthin from edible brown algae Sargassum fusiforme using different green solvents was presented. Ethyl lactate, limonene, soybean oil, and sunflower oil were used in place of traditional organic solvents. Ethyl lactate showed similar performance to organic solvents, whereas limonene and vegetable oil exhibited higher selectivity for fucoxanthin. Moreover, the effects of various extraction factors, including liquid/solid ratio, extraction time, extraction temperature, as well as amplitude were studied. The optimal conditions were optimized as follows: liquid/solid ratio, 40 mL/g; extraction time, 27 min; extraction temperature, 75 ℃; amplitude, 53%; and solvent, ethyl lactate. Optimal model of second-order kinetic parameters (rate constant, equilibrium concentration, and initial extraction rate) was successfully developed for describing the dynamic ultrasonic extraction process under different operating conditions.     

Ultrasound-assisted alkaline proteinase extraction enhances the yield of pecan protein and modifies its functional properties

To enhance the extraction yield of pecan protein and modify its functional properties, this study investigated whether both ultrasound and enzyme have a synergistic impact on the extraction of pecan (Carya illinoinensis (Wangenh.) K. Koch) protein. The highest protein extraction rate (25.51%) was obtained under the conditions of 1415.43 W^.cm⁻², 15 min, pH 10.0, 50 °C, and 1% (w/w) alkaline proteinase. Owing to its high shear, mechanical energy and cavitation, the ultrasound process increased the solubility of the substrate making it readily accessible to the enzyme, thereby accelerating the chemical reaction and improving the yield of the protein. The optimized ultrasound-assisted enzymatic method (400 W, 20 kHz, 5 s/3s) effectively changed the secondary and tertiary structure of the pecan protein. The results of surface hydrophobicity, intrinsic fluorescence spectra, sulfhydryl content and scanning electron microscopy all indicated the unfolding of protein and exposure of hydrophobic groups and sulfhydryl groups. Moreover, the protein obtained by this method showed higher solubility (70.77%), higher emulsifying activity (120.56 m²/g), smaller particle size (326.7 nm), and better dispersion (0.305) than single ultrasound and non-ultrasound methods (p < 0.05). To conclude, ultrasound-assisted enzymatic method could be an appropriate technique to improve the yield and quality of the pecan protein. The study also provides a theoretical basis for the application of pecan protein in food processing.     

Direct enrichment of olive oil in oleuropein by ultrasound-assisted maceration at laboratory and pilot plant scale

The possibility to improve the nutritional value of olive oil by enriching it in phenolic compounds from olive leaves (e.g., oleuropein) by ultrasonic maceration was studied. The experimental design used led to the following optimal extraction conditions: ultrasonic power of 60 W, temperature of 16 °C and sonication duration of 45 min. The high total phenolic content (414.3 ± 3.2 mg of oleuropein equivalent/kg of oil), oleuropein (111.0 ± 2.2 mg/kg of oil) and α-tocopherol (55.0 ± 2.1 g/kg of oil) concentrations obtained by optimized ultrasound-assisted extraction (UAE) proved the efficiency of this process when compared with the conventional solid-liquid extraction. Histochemical analyses showed that this efficiency is due to specific alteration of the phenol-containing leaf structures. Furthermore, the radical-scavenging activity of the processed oil (DPPH test) and its stability toward lipid autoxidation (heating test) confirmed its enrichment in antioxidants. Sensory evaluation of the enriched olive oil showed a slight increase in bitterness but an overall acceptability. Finally, the enriched olive oil was characterized by clear green color (L^∗, a^∗, b^∗ parameters).     

Structural and hydrophobic-hydrophilic properties of nanosilica/zirconia alone and with adsorbed PDMS

Two nanosilica A-300/zirconia (SZ) composites at zirconia content CZrO₂=5 and 20 wt.% were synthesized using a wet impregnation method with zirconium acetylacetonate as a precursor. The specific surface area of SZ is larger than that of A-300 because zirconia is composed of nanoparticles (crystallites of 4 nm in average size at CZrO₂=20 wt.%) smaller than those of the initial silica (d_av ≈ 11 nm). A-300 and SZ modified by polydimethylsiloxane (PDMS at molecular weight 1700 and 7960) in amounts of 5, 10, 15, 20 and 40 wt.% remained in the powder state with aggregates of primary particles smaller than those of A-300. SZ is more hydrophilic than silica but PDMS/SZ is more hydrophobic (maximum hydrophobic at C_PDMS 15-20 or 40 wt.%) than PDMS/A-300.     

Electric conduction properties of M@C2n endohedral metallofullerenes (M=La, Y)

The electrical conduction properties of powder samples of M@C_2n endohedral metallofullerenes (M=La, Y) isolated from soot by extraction with N,N-dimethylformamide and by sublimation were studied. It was established that the conductivity of sublimated samples exceeded that of the extracted ones by four orders of magnitude and was as high as 0.2–0.5 Ω^?1 cm^?1 at room temperature.